CN112378722B - Aluminum/transition layer/lead alloy/PbO 2 Rapid preparation method of metallographic sample of composite rod - Google Patents
Aluminum/transition layer/lead alloy/PbO 2 Rapid preparation method of metallographic sample of composite rod Download PDFInfo
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- CN112378722B CN112378722B CN202011279662.9A CN202011279662A CN112378722B CN 112378722 B CN112378722 B CN 112378722B CN 202011279662 A CN202011279662 A CN 202011279662A CN 112378722 B CN112378722 B CN 112378722B
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- 229910000978 Pb alloy Inorganic materials 0.000 title claims abstract description 99
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 85
- 230000007704 transition Effects 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000005498 polishing Methods 0.000 claims abstract description 103
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 244000137852 Petrea volubilis Species 0.000 claims description 27
- 239000000839 emulsion Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000003599 detergent Substances 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 239000003822 epoxy resin Substances 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000002649 leather substitute Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- 229910014474 Ca-Sn Inorganic materials 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 125000003916 ethylene diamine group Chemical group 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 239000000919 ceramic Substances 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000005520 cutting process Methods 0.000 abstract description 3
- 239000003607 modifier Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 69
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 44
- 229910001278 Sr alloy Inorganic materials 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 10
- IZJSTXINDUKPRP-UHFFFAOYSA-N aluminum lead Chemical compound [Al].[Pb] IZJSTXINDUKPRP-UHFFFAOYSA-N 0.000 description 6
- 238000007747 plating Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229960001124 trientine Drugs 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical compound [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an aluminum/transition layer/lead alloy/PbO 2 A rapid preparation method of a metallographic sample of a composite rod belongs to the technical fields of metallographic detection and sample preparation. The method comprises cutting rod-shaped aluminum/transition layer/lead alloy/PbO 2 Sample is subjected to the procedures of sample embedding, mechanical grinding, fine polishing, electrolytic chemical compound polishing and the like to prepare the aluminum/transition layer/lead alloy/PbO 2 Metallographic phase sample of the composite rod. The invention relates to an aluminum/transition layer/lead alloy/PbO 2 The metallographic sample of the composite rod has clear aluminum/transition layer/lead alloy and lead alloy/PbO 2 The interface morphology of the lead alloy and the real metallographic structure of the lead alloy; the method has simple operation and does not damage the ceramic layer PbO 2 The structure is short in sample preparation time, high in working efficiency, high in definition of prepared sample structure, and particularly suitable for comprehensive detection of interface combination compactness of a composite rod of the aluminum-based lead alloy conductive ceramic film and metallographic structure of modifier elements in the lead alloy, so that the performance of the composite material is accurately judged.
Description
Technical Field
The invention relates to an aluminum/transition layer/lead alloy/PbO 2 A rapid preparation method of a metallographic sample of a composite rod belongs to the technical fields of metallographic detection and sample preparation.
Background
At present, most methods for embedding and manufacturing metallographic samples comprise a high-temperature heat-resistant automatic embedding machine and dental tray powder, or clamping by a clamp for sample manufacturing. The clamp can loosen, slip and the like in the sample polishing process, so that the sample preparation effect is affected; the dental tray powder is used for inlaying, and the main component of the dental tray powder is methyl methacrylate, so that the dental tray powder has low strength and brittleness, is easy to abrade when a sample is polished, and generates pores between the dental tray powder and the sample, so that the smoothness and the cleaning of the sample are not facilitated; meanwhile, the inside of the sample is loose, porous and non-conductive, the sample can not be directly used for detection by a scanning electron microscope, scratches are easy to generate in the process of taking out the sample, and the detection effect is affected. Although the high-temperature heat-resistant automatic inlay machine has high sample preparation efficiency, the interface structure of aluminum and lead alloy and the interface structure of lead alloy and lead dioxide are easily damaged due to the difference of thermal expansion coefficients, and the sample preparation cost is high.
Aluminum has low bending strength, light weight, good conductivity and low cost relative to lead alloy, while lead alloy has poor conductivity and creep resistance but better corrosion resistance in sulfuric acid medium solution of nonferrous metal electrodeposition, the two materials are directly combined and applied to generate higher interfacial resistance due to large difference of linear expansion coefficients, and aluminum and lead are in an immiscible system, and the thermodynamic mixing enthalpy delta Hmax of the aluminum and the lead is higher than that of the lead>0, it is difficult to directly synthesize the aluminum-lead alloy composite material by adopting the traditional method, so that the preparation of the novel aluminum-lead layered composite electrode material is very necessary. In addition, pbO grows on the surface of the lead alloy in situ due to common problems of high oxygen evolution overpotential, poor fluorine-chlorine ion corrosion resistance and the like of the surface of the lead alloy 2 Preparation of aluminum/transition layer/lead alloy/PbO for nonferrous metal electro-deposition by film 2 The composite anode plate is widely concerned, the structure of the aluminum/transition layer/lead alloy and the lead alloy and lead dioxide layer in the composite rod is observed under microscopic observation, and the research on the influence of the change rule of the structure on the anode performance is practically significant.
The lead and lead alloy is soft, has small hardness, weak ductility and strong expansibility, the surface in the air is easy to oxidize, the hardness of the aluminum and the aluminum alloy is also lower, uneven force is applied in the grinding and polishing process, uneven grinding surfaces are easily caused, and uneven grinding surfaces are caused. The composite rod material has the advantages that the flow of the lead surface layer is large in the intercepting and polishing processes, a deformation layer is easy to cover the real tissues of the composite rod material, the lead alloy is easy to generate heat and recrystallize in the processes, is easy to oxidize and cover the real tissues of the lead alloy, more silicon carbide particles are embedded in the process of grinding the composite rod for a longer time or with larger force, a certain confusion is caused on the observation of secondary phases and intermetallic compounds in the lead alloy, the secondary phases and the intermetallic compounds are difficult to observe, the surface deformation layer, the oxidation layer and a large number of silicon carbide particles cover the real tissue morphology or the interface morphology, and the combination quality of the aluminum-lead alloy composite material and the real tissue structure of the lead alloy cannot be accurately estimated. How fast to eliminate artefacts is particularly important.
Therefore, there is a need to develop an aluminum/transition layer/lead alloy/PbO which is simple, convenient and safe, does not damage the structure of the ceramic lead dioxide layer, and ensures that the observed metallographic phase is a real structure or a real morphology 2 A method for quickly preparing a composite rod inlaid pattern and a metallographic phase.
Disclosure of Invention
The invention aims at the prior art of aluminum/transition layer/lead alloy/PbO 2 The problem of preparation of a metallographic sample of a composite rod is that an aluminum/transition layer/lead alloy/PbO is provided 2 The invention relates to a rapid preparation method of a metallographic sample of a composite rod, which prepares aluminum/transition layer/lead alloy and lead alloy/PbO 2 The method has simple operation and does not damage the PbO of the ceramic layer 2 The structure is short in sample preparation time, high in working efficiency, high in definition of prepared sample structure, and particularly suitable for comprehensive detection of interface bonding compactness of a composite rod of an aluminum/transition layer/lead alloy conductive ceramic film and a modifier element metallographic structure in a lead alloy, so that the performance of the composite material is accurately judged, and the problem of mass quality caused by an anode of the composite rod in subsequent wet electrometallurgical process is avoided.
Aluminum/transition layer/lead alloy/PbO 2 The rapid preparation method of the metallographic sample of the composite rod comprises the following specific steps:
(1) Intercepting a sample: intercepting rod-shaped aluminum/transition layer/lead alloy/PbO under the cooling of emulsion 2 The sample is washed by adopting a metal detergent and water in sequence, and is dried by cold air;
(2) Inlay sample: the rod-shaped aluminum/transition layer/lead alloy/PbO in the step (1) 2 The side of the sample was perforated, an electrically conductive copper wire was connected to the sample aluminum core, and a rod-like aluminum/transition layer/lead alloy/PbO was used 2 Placing the sample into a mold, extending the end of the conductive copper wire out of the silica gel mold, pouring the liquid mosaic material into the mold until the liquid mosaic material is completely immersed to cover the rod-shaped aluminum/transition layer/lead alloy/PbO 2 Solidifying the sample at room temperature, and demoulding to obtain a cold mosaic sample with a conductive wire;
(3) Mechanical grinding: two kinds of silicon carbide waterproof abrasive paper with different thicknesses are stuck on the same metallographic polishing machine disc, the cold mosaic sample with the conductive wire in the step (2) is subjected to mechanical polishing through 320#/400# waterproof abrasive paper, 600#/800# waterproof abrasive paper, 1000#/1200# waterproof abrasive paper and 1500# waterproof abrasive paper combined with 2000# waterproof abrasive paper, 20-70% of ethanol solution is dripped during the mechanical polishing, and the polished cold mosaic sample is placed in 40-70% of ethanol solution for ultrasonic cleaning and is dried by cold air;
(4) Fine polishing: coarsely polishing the cold mosaic sample polished in the step (3) on a high polymer synthetic leather polishing cloth for 1-5 min, and finely polishing on a golden velvet polishing cloth for 1-2 min to make the polished surface smooth and bright like a mirror, wherein the grain size of the polishing agent is 0.01-1 mu m;
(5) Electrolytic chemical composite polishing: taking the finely polished cold mosaic sample in the step (4) as an anode, taking a polishing disk as a cathode, and carrying out electrolytic chemical compound polishing in a direct current loop formed by polishing fabrics containing electrolyte for 5-60S to obtain the aluminum/transition layer/lead alloy/PbO 2 Metallographic phase sample of the composite rod.
The step (1) is a rod-shaped aluminum/transition layer/lead alloy/PbO 2 The sample is a round bar or an elliptic bar, the diameter of the round bar is 4-18 mm, the major axis of the elliptic bar is 10-100 mm, the minor axis is 4-18 mm, the round diameter of the section of the aluminum core is 2-12 mm, the major axis of the elliptic bar is 4-80 mm, the minor axis is 2-10 mm, the thickness of the lead alloy layer is 0.5-10 mm, and the thickness of the PbO 2 The thickness of the layer is 10-3000 μm.
The transition layer in the step (1) is an alloy composed of two or more than two of Cu, ni, ag, zn and Cu, ni, ag, zn, and the thickness is 0.5-30 mu m; the lead alloy is one or more of Pb-Ag-Ca-Sn, pb-Ag-Sn-Sr-Sb, pb-Ag-Ca-Sr-rare earth, pb-Ag-Sn-Sr-Sb-rare earth.
The emulsion in the step (1) is a mixed solution of the emulsion and deionized water, and the mass concentration of the emulsion in the emulsion is 1.5-5%; the metal detergent is a water-based metal detergent and is purchased from Kunming gantry daily use washing liability company.
The liquid mosaic sample in the step (2) contains 50-90 wt% of epoxy resin powder, 10-30 wt% of curing agent and 10-20 wt% of diluent in percentage by mass.
Further, the epoxy resin is E44 or E51, and the particle size of the epoxy resin is 1-10 mu m; the curing agent is ethylenediamine, diethylenetriamine, triethylenetetramine or polyamide; the diluent is epoxy diluent 692, butanediol diepoxide, toluene or xylene.
The step (3) is that the coarse sand paper in two kinds of silicon carbide water sand papers with different thickness on the same metallographic polishing machine disc is a ring and is stuck to the edge of the grinding disc, and the outer diameter is 150 mm-300 mm; the fine sand paper is round and is attached to the center of the grinding disc, and the diameter of the fine sand paper is 100-150 mm.
The polishing agent in the step (4) is a diamond spray, an aluminum oxide polishing solution or a silicon dioxide polishing solution.
And (5) the cathode polishing disc in the step is a conductive carbon fiber, aluminum disc, copper disc or stainless steel disc.
The electrolyte in the step (5) contains 10-20% of perchloric acid, 20-50% of glacial acetic acid, 30-50% of ethanol and 10-50% of deionized water by volume percentage; the voltage of the electrolytic chemical compound polishing is 2-4V, and the temperature is 0-20 ℃.
The beneficial effects of the invention are as follows:
(1) The invention adopts cold mosaic sample, has short curing time, small heat release and high sample preparation efficiency; the whole process is simple to operate, does not damage the lead dioxide organization structure of the polar plate ceramic membrane, and is safe and reliable;
(2) According to the invention, two kinds of silicon carbide waterproof abrasive paper with different thicknesses are adhered on the same metallographic polishing machine disc, so that polishing efficiency and polishing quality can be improved;
(3) The adoption of the hard transition layer Cu, ni, ag, zn and the alloy formed by the hard transition layer Cu, ni, ag, zn can greatly improve the binding force between aluminum and lead alloy and can obtain a very clear interface tissue structure;
(4) According to the invention, alcohol polishing, cooling and lubrication are adopted, so that the polished surface of the sample is smooth, and the ultrasonic waves can be used for efficiently cleaning impurity particles embedded in the lead alloy;
(5) Aluminum/transition layer/lead alloy/PbO 2 Four different plating intermediate lead alloy layers of composite rodThe invention adopts electrolytic chemical compound polishing, has short time, and can clearly display the morphology of an aluminum-transition layer-lead interface, a lead and lead dioxide interface and the real metallographic structure of a lead alloy.
Drawings
FIG. 1 shows an aluminum/transition layer/lead alloy/PbO 2 A process flow chart for embedding the composite rod sample;
FIG. 2 is a cross-sectional view of the silicone mold after embedding the sample; wherein the 1-aluminum/transition layer, the 2-lead alloy, and the 3-PbO 2 4-mounting material, 5-conductive copper wires and 6-silica gel;
FIG. 3 is a graph of the interface morphology of the aluminum/tin/Pb-Ag-Ca-Sr alloy of example 1;
FIG. 4 is a graph showing the interface morphology of the aluminum/nickel/Pb-Ag-Ca-Sr alloy of example 2;
FIG. 5 is a graph showing the interface morphology of the aluminum/copper/Pb-Ag-Ca-Sr alloy of example 3;
FIG. 6 is a diagram of example 3Pb-Ag-Ca-Sr/PbO 2 An interface morphology graph;
FIG. 7 is a diagram of the Pb-Ag-Ca-Sr alloy according to example 3.
Detailed Description
The invention will be described in further detail with reference to specific embodiments, but the scope of the invention is not limited to the description.
Example 1: aluminum/transition layer/lead alloy/PbO 2 The rapid preparation method of the metallographic sample of the composite rod (see figure 1) comprises the following specific steps:
(1) Intercepting a sample: under the cooling of the emulsion, a linear cutting machine is adopted to cut the rod-shaped aluminum/transition layer/lead alloy/PbO at the speed of 0.4mm/S 2 The sample is washed by adopting a metal detergent and water in sequence, and is dried by cold air; wherein the emulsion is a mixed solution of special emulsion paste for wire feeding in the kernel light and deionized water, and the mass concentration of the emulsion paste in the emulsion is 2.44%; the metal detergent is a Lijie brand water-based metal detergent of Kunming gantry daily-use washing limited liability company; aluminum/transition layer/lead alloy/PbO 2 The sample is a round bar, the diameter of the round bar is 12mm, the diameter of the aluminum core is 6mm, the lead alloy is Pb-Ag-Ca-Sr, the thickness is about 3mm, and the aluminum-lead alloy is added withThe transition layer tin layer is about 5 mu m, and the round bar is 20mm long;
(2) Mosaic sample (see fig. 1): the rod-shaped aluminum/transition layer/lead alloy/PbO in the step (1) 2 The side of the sample was perforated, an electrically conductive copper wire was connected to the sample aluminum core, and a rod-like aluminum/transition layer/lead alloy/PbO was used 2 Placing the sample into a mold, extending the end of the conductive copper wire out of the silica gel mold, pouring the liquid mosaic material into the mold until the liquid mosaic material is completely immersed to cover the rod-shaped aluminum/transition layer/lead alloy/PbO 2 The sample is solidified for 5 minutes at room temperature, and the section view of the silica gel mold after embedding the sample is shown in fig. 2; demoulding to obtain a cold mosaic sample with a conductive wire; wherein the liquid mosaic material contains 60% of epoxy resin powder (E44 epoxy resin powder with the particle size of 5 mu m), 25% of curing agent (ethylenediamine) and 15% of diluent (epoxy diluent 692) in percentage by mass;
(3) Mechanical grinding: two kinds of silicon carbide waterproof abrasive paper with different thickness are stuck on the same metallographic polishing machine disc, wherein the coarse abrasive paper is in a ring shape and stuck on the edge of the grinding disc, and the outer diameter is 300mm; the fine sand paper is round and is stuck to the center of the grinding disc, and the diameter of the fine sand paper is 100mm; mechanically polishing the cold mosaic sample with the conductive wire in the step (2) through water sand paper combined with 320# 400# 600# 800# 1000# 1200# 1500# 2000, wherein the polishing speed is 500 revolutions per minute, the coarse sand paper is firstly thick and then thin, one sand paper is replaced each time, 90 degrees of rotation is carried out, 50% ethanol solution is dropwise added while the mechanical polishing is carried out, the polished cold mosaic sample is placed in 60% ethanol solution, ultrasonic cleaning is carried out for 3min, and cold air drying is carried out;
(4) Fine polishing: coarsely polishing the cold mosaic sample polished in the step (3) on a high molecular synthetic leather polishing cloth for 2min, and finely polishing the cold mosaic sample on a golden silk velvet polishing cloth for 2min to ensure that the polished surface is free from scratches and bright like a mirror, wherein the finely polished polishing agent is a mixture of a diamond spray and 5wt% of deionized water, and the particle size of the diamond spray is 0.5 mu m; during polishing, the grinding surface of the sample and the polishing disk are ensured to be parallel and uniformly lightly pressed on the polishing disk;
(5) Electrolytic chemical composite polishing: taking the finely polished cold mosaic sample in the step (4) as an anode, taking a polishing disk (aluminum disk) as a cathode, and feeding the sample into a direct current loop formed by polishing fabrics containing electrolyteCarrying out electrolytic chemical compound polishing for 20S to obtain the aluminum/transition layer/lead alloy/PbO 2 A metallographic sample of the composite rod; wherein the electrolyte contains 15% perchloric acid, 30% glacial acetic acid, 40% ethanol and 15% deionized water by volume percent; the voltage of electrolytic chemical compound polishing is 4V, and the temperature is 10 ℃;
in the embodiment, the interface morphology diagram of the aluminum/tin/Pb-Ag-Ca-Sr alloy is shown in fig. 3, and the interface combination condition of the aluminum and the Pb-Ag-Ca-Sr alloy can be clearly seen from fig. 3, and the tin and the lead alloy are better compounded in most areas at the interface, but are poorer in combination with the aluminum, and most positions have defects.
Example 2: aluminum/transition layer/lead alloy/PbO 2 The rapid preparation method of the metallographic sample of the composite rod (see figure 1) comprises the following specific steps:
(1) Intercepting a sample: under the cooling of the emulsion, a linear cutting machine is adopted to cut the rod-shaped aluminum/transition layer/lead alloy/PbO at the speed of 0.5mm/S 2 The sample is washed by adopting a metal detergent and water in sequence, and is dried by cold air; wherein the emulsion is a mixed solution of special emulsion paste for wire feeding in the kernel light and deionized water, and the mass concentration of the emulsion paste in the emulsion is 1.96%; the metal detergent is Lijie brand water-based metal detergent of Kunming gantry daily washing limited liability company, aluminum/transition layer/lead alloy/PbO 2 The sample is a round bar, the diameter of the round bar is 12.5mm, the diameter of the aluminum core is 6mm, a transition layer nickel layer is added in the aluminum-lead alloy, the nickel layer is about 4 mu m, and the length of the round bar is 20mm;
(2) Mosaic sample (see fig. 1): the rod-shaped aluminum/transition layer/lead alloy/PbO in the step (1) 2 The side of the sample was perforated, an electrically conductive copper wire was connected to the sample aluminum core, and a rod-like aluminum/transition layer/lead alloy/PbO was used 2 Placing the sample into a mold, extending the end of the conductive copper wire out of the silica gel mold, pouring the liquid mosaic material into the mold until the liquid mosaic material is completely immersed to cover the rod-shaped aluminum/transition layer/lead alloy/PbO 2 The sample is solidified for 2 minutes at room temperature, and the section view of the silica gel mold after embedding the sample is shown in fig. 2; demoulding to obtain a cold mosaic sample with a conductive wire; wherein the liquid mosaic sample comprises 60% of epoxy resin powder (E51 epoxy resin powder with the particle diameter of 1 μm), 25% of curing agent (diethylenetriamine) and 15% of dilutionAgents (butanediol bisepoxy);
(3) Mechanical grinding: two kinds of silicon carbide water sand paper with different thickness are stuck on the same metallographic polishing machine disc, wherein the coarse sand paper is in a ring shape and stuck on the edge of the grinding disc, and the outer diameter is 300mm; the fine sand paper is round and is stuck to the center of the grinding disc, and the diameter of the fine sand paper is 150mm; mechanically polishing the cold mosaic sample with the conductive wire in the step (2) through water sand paper combined with 320# 400# 600# 800# 1000# 1200# 1500# 2000, wherein the polishing speed is 600 revolutions per minute, the coarse sand paper is firstly thick and then thin, one sand paper is replaced each time, 90 degrees of rotation is carried out, 60% ethanol solution is dropwise added while the mechanical polishing is carried out, the polished cold mosaic sample is placed in the 60% ethanol solution, ultrasonic cleaning is carried out for 3min, and cold air drying is carried out;
(4) Fine polishing: coarsely polishing the cold mosaic sample polished in the step (3) on a high molecular synthetic leather polishing cloth for 3min, and finely polishing the cold mosaic sample on a golden silk velvet polishing cloth for 2min to ensure that the polished surface is free from scratches and bright like a mirror, wherein the finely polished polishing agent is a mixture of an aluminum oxide polishing solution and 10wt% of deionized water, and the grain size of the aluminum oxide polishing solution is 1 mu m; during polishing, the grinding surface of the sample and the polishing disk are ensured to be parallel and uniformly lightly pressed on the polishing disk;
(5) Electrolytic chemical composite polishing: taking the finely polished cold mosaic sample in the step (4) as an anode, taking a polishing disk (aluminum disk) as a cathode, and carrying out electrolytic chemical compound polishing in a direct current loop formed by polishing fabrics containing electrolyte for 10 seconds to obtain the aluminum/transition layer/lead alloy/PbO 2 A metallographic sample of the composite rod; wherein the electrolyte contains 25% perchloric acid, 30% glacial acetic acid, 35% ethanol and 15% deionized water by volume percent; the voltage of electrolytic chemical compound polishing is 3.5V, and the temperature is 16 ℃;
the interface morphology diagram of the aluminum/nickel/Pb-Ag-Ca-Sr alloy in the embodiment is shown in fig. 4, the interface combination condition of the plating layer and the aluminum and Pb-Ag-Ca-Sr alloy can be clearly seen from fig. 4, the nickel plating layer and the aluminum matrix are better in metallurgical combination, and meanwhile, the plating layer and the lead alloy are better in combination, and no obvious defect exists, so that the combination defect between the lead alloy and the aluminum matrix is reduced.
Example 3: aluminum/transition layer/lead alloy/PbO 2 Metallographic phase of composite rodThe sample rapid preparation method (see figure 1) comprises the following specific steps:
(1) Intercepting a sample: under the cooling of the emulsion, a linear cutter is adopted to intercept rod-shaped aluminum/transition layer/lead alloy/PbO at the speed of 0.4mm/s 2 The sample is washed by adopting a metal detergent and water in sequence, and is dried by cold air; wherein the emulsion is a mixed solution of special emulsion paste for wire feeding in the kernel light and deionized water, and the mass concentration of the emulsion paste in the emulsion is 2.17%; the metal detergent is Lijie brand water-based metal detergent of Kunming gantry daily washing limited liability company, aluminum/transition layer/lead alloy/PbO 2 The sample is an elliptic rod, the major axis of the elliptic rod is 50mm, the minor axis is 10mm, the major axis of the aluminum core is 40mm, the minor axis is 6mm, and PbO 2 The layer is 60 μm; a transition layer copper layer is added in the aluminum-lead alloy, and the copper layer is about 2 mu m;
(2) Mosaic sample (see fig. 1): the rod-shaped aluminum/transition layer/lead alloy/PbO in the step (1) 2 The side of the sample was perforated, an electrically conductive copper wire was connected to the sample aluminum core, and a rod-like aluminum/transition layer/lead alloy/PbO was used 2 Placing the sample into a mold, extending the end of the conductive copper wire out of the silica gel mold, pouring the liquid mosaic material into the mold until the liquid mosaic material is completely immersed to cover the rod-shaped aluminum/transition layer/lead alloy/PbO 2 The sample is solidified for 5 minutes at room temperature, and the section view of the silica gel mold after embedding the sample is shown in fig. 2; demoulding to obtain a cold mosaic sample with a conductive wire; wherein the liquid mosaic sample contains 65% of epoxy resin powder (E51 epoxy resin powder with the particle size of 1 mu m), 25% of curing agent (triethylene tetramine) and 10% of diluent (dimethylbenzene) in percentage by mass;
(3) Mechanical grinding: two kinds of silicon carbide water sand paper with different thickness are stuck on the same metallographic polishing machine disc, wherein the coarse sand paper is in a ring shape and stuck on the edge of the grinding disc, and the outer diameter is 300mm; the fine sand paper is round and is stuck to the center of the grinding disc, and the diameter of the fine sand paper is 150mm; mechanically polishing the cold mosaic sample with the conductive wire in the step (2) through water sand paper combined with 320# 400# 600# 800# 1000# 1200# 1500# 2000, wherein the polishing speed is 500 revolutions per minute, the coarse sand paper is firstly thick and then thin, one sand paper is replaced each time, 90 degrees of rotation is carried out, 50% ethanol solution is dropwise added while the mechanical polishing is carried out, the polished cold mosaic sample is placed in the 50% ethanol solution for ultrasonic cleaning for 3min, and the cold air is dried;
(4) Fine polishing: coarsely polishing the cold mosaic sample polished in the step (3) on a high molecular synthetic leather polishing cloth for 2min, and finely polishing on a golden velvet polishing cloth for 1min to ensure that the polished surface is free from scratches and bright like a mirror, wherein the finely polished polishing agent is a mixture of silicon dioxide polishing solution and 10wt% of deionized water, and the particle size of the silicon dioxide polishing solution is 0.5 mu m; during polishing, the grinding surface of the sample and the polishing disk are ensured to be parallel and uniformly lightly pressed on the polishing disk;
(5) Electrolytic chemical composite polishing: taking the finely polished cold mosaic sample in the step (4) as an anode, taking a polishing disk (aluminum disk) as a cathode, and carrying out electrolytic chemical compound polishing for 45S in a direct current loop formed by polishing fabrics containing electrolyte to obtain the aluminum/transition layer/lead alloy/PbO 2 A metallographic sample of the composite rod; wherein the electrolyte contains 25% perchloric acid, 40% glacial acetic acid, 25% ethanol and 10% deionized water by volume percent; the voltage of electrolytic chemical compound polishing is 4V, and the temperature is 15 ℃;
the interface morphology diagram of the aluminum/copper/Pb-Ag-Ca-Sr alloy in the embodiment is shown in fig. 5, the interface combination condition of the plating layer and the aluminum and Pb-Ag-Ca-Sr alloy can be clearly seen from fig. 5, the metallurgical combination of the copper plating layer and the aluminum substrate is better, the cladding layer and the lead alloy are better composited, and no obvious defect exists, so that the combination defect between the lead alloy and the aluminum substrate is reduced; pb-Ag-Ca-Sr/PbO 2 The interface morphology is shown in FIG. 6, and the PbO deposited by Pb-Ag-Ca-Sr alloy is clearly seen from FIG. 6 2 Film layer, pbO 2 The film layer is uniform and compact and has uniform thickness; the Pb-Ag-Ca-Sr alloy gold phase diagram is shown in FIG. 7, and the clear lead alloy grains can be seen from FIG. 7, the grain structure growth is distributed along the central aluminum matrix in a ring shape, the grains are extruded more obviously closer to the central grains, the grains are finer, and the peripheral grains are relatively coarse.
While the present invention has been described in detail with reference to the specific embodiments, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (8)
1. Aluminum/transition layer/lead alloy/PbO 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following specific steps:
(1) Intercepting a sample: intercepting rod-shaped aluminum/transition layer/lead alloy/PbO under the cooling of emulsion 2 The sample is washed by adopting a metal detergent and water in sequence, and is dried by cold air; the transition layer is Cu, ni, ag or Zn or an alloy composed of more than two kinds, and the thickness is 0.5-30 mu m; the lead alloy is one or more of Pb-Ag-Ca-Sn, pb-Ag-Sn-Sr-Sb, pb-Ag-Ca-Sr-rare earth, pb-Ag-Sn-Sr-Sb-rare earth;
(2) Inlay sample: the rod-shaped aluminum/transition layer/lead alloy/PbO in the step (1) 2 The side of the sample was perforated, an electrically conductive copper wire was connected to the sample aluminum core, and a rod-like aluminum/transition layer/lead alloy/PbO was used 2 Placing the sample into a mold, extending the end of the conductive copper wire out of the silica gel mold, pouring the liquid mosaic material into the mold until the liquid mosaic material is completely immersed to cover the rod-shaped aluminum/transition layer/lead alloy/PbO 2 Solidifying the sample at room temperature, and demoulding to obtain a cold mosaic sample with a conductive wire;
(3) Mechanical grinding: two kinds of silicon carbide waterproof abrasive paper with different thicknesses are stuck on the same metallographic polishing machine disc, the cold mosaic sample with the conductive wire in the step (2) is subjected to mechanical polishing through 320#/400# waterproof abrasive paper, 600#/800# waterproof abrasive paper, 1000#/1200# waterproof abrasive paper and 1500# waterproof abrasive paper combined with 2000# waterproof abrasive paper, 20-70% of ethanol solution is dripped during the mechanical polishing, and the polished cold mosaic sample is placed in 40-70% of ethanol solution for ultrasonic cleaning and is dried by cold air;
(4) Fine polishing: coarsely polishing the cold mosaic sample polished in the step (3) on a high polymer synthetic leather polishing cloth for 1-5 min, and finely polishing on a golden velvet polishing cloth for 1-2 min, wherein the grain size of the polishing agent is 0.01-1 mu m;
(5) Electrolytic chemical composite polishing: taking the finely polished cold mosaic sample in the step (4) as an anode, taking a polishing disk as a cathode, and carrying out electrolytic chemical compound polishing in a direct current loop formed by polishing fabrics containing electrolyte for 5-60S to obtain the aluminum/transition layer/lead alloy/PbO 2 A metallographic sample of the composite rod;
the electrolyte contains 10-20% of perchloric acid, 20-50% of glacial acetic acid, 10-30% of citric acid, 30-50% of ethanol and 10-50% of deionized water in percentage by mass; the voltage of the electrolytic chemical compound polishing is 2-4V, and the temperature is 0-20 ℃.
2. The aluminum/transition layer/lead alloy/PbO of claim 1 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: step (1) rod-shaped aluminum/transition layer/lead alloy/PbO 2 The sample is a round bar or an elliptic bar, the diameter of the round bar is 4-18 mm, the major axis of the elliptic bar is 10-100 mm, the minor axis is 4-18 mm, the round diameter of the section of the aluminum core is 2-12 mm, the major axis of the elliptic bar is 4-80 mm, the minor axis is 2-10 mm, the thickness of the lead alloy layer is 0.5-10 mm, and the thickness of the PbO 2 The thickness of the layer is 10-3000 μm.
3. The aluminum/transition layer/lead alloy/PbO of claim 1 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: the emulsion in the step (1) is a mixed solution of the emulsion and deionized water, and the mass concentration of the emulsion in the emulsion is 1.5-5%; the metal detergent is water-based metal detergent.
4. The aluminum/transition layer/lead alloy/PbO of claim 1 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: the liquid mosaic sample in the step (2) contains 50-90 wt% of epoxy resin powder, 10-30 wt% of curing agent and 10-20 wt% of diluent in percentage by mass.
5. The aluminum/transition layer/lead alloy/PbO of claim 4 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: the epoxy resin is E44 or E51, and the particle size of the epoxy resin is 1-10 mu m; the curing agent is ethylenediamine, diethylenetriamine, triethylenetetramine or polyamide; the diluent is epoxy diluent 692, butanediol diepoxide, toluene or xylene.
6. The aluminum/transition of claim 1Layer/lead alloy/PbO 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: the step (3) is that the coarse sand paper in two kinds of silicon carbide water sand papers with different thickness on the same metallographic polishing machine disc is circular and stuck to the edge of the grinding disc, and the outer diameter is 150 mm-300 mm; the fine sand paper is round and is attached to the center of the grinding disc, and the diameter of the fine sand paper is 100-150 mm.
7. The aluminum/transition layer/lead alloy/PbO of claim 1 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: the polishing agent in the step (4) is a diamond spray, an aluminum oxide polishing solution or a silicon dioxide polishing solution.
8. The aluminum/transition layer/lead alloy/PbO of claim 1 2 The rapid preparation method of the metallographic sample of the composite rod is characterized by comprising the following steps of: and (5) the cathode polishing disc is a conductive carbon fiber disc, an aluminum disc, a copper disc or a stainless steel disc.
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